Agilent infinitylab lc series diode array detector wr and multiple wavelength detector (g7115a g7165a) user manual

Agilent InfinityLab LC Series

Diode Array Detector WR
and Multiple Wavelength
Detector

User Manual

Agilent Technologies


Notices
© Agilent Technologies, Inc. 2016-2018

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document that conflict with these
terms, the warranty terms in the separate agreement shall control.

Manual Part Number
G7115-90000 Rev. B

Edition
03/2018
Printed in Germany
Agilent Technologies
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76337 Waldbronn

receive no greater than Restricted Rights as
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1987). U.S. Government users will receive
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applicable in any technical data.

Safety Notices

C AU T I O N
A CAUTION notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly performed or adhered to, could
result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION
notice until the indicated conditions are fully understood and
met.

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The hardware and/or software described in
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defined in DFAR 252.227-7014 (June 1995),
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WA R N I N G
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice,
or the like that, if not correctly
performed or adhered to, could
result in personal injury or
death. Do not proceed beyond a
WARNING notice until the indicated conditions are fully
understood and met.

Agilent InfinityLab LC Series DAD WR and MWD User Manual


In This Guide...

In This Guide...

This manual covers the Agilent 1260 Infinity II Diode Array Detector WR and
the Agilent 1260 Infinity II Multiple Wavelength Detector modules:
• G7115A - 1260 Infinity II DAD WR
• G7165A - 1260 Infinity II MWD

1 Introduction
This chapter gives an introduction to the module.

2 Site Requirements and Specifications
This chapter provides information on environmental requirements, physical
and performance specifications.

3 Using the Module
This chapter explains the essential operational parameters of the module.

4 Preparing the Detector
This chapter provides information on how to set up the module for an analysis
and explains the basic settings.

5 Optimizing the Detector
This chapter provides information on how to optimize the detector.

6 Troubleshooting and Diagnostics
This chapter gives an overview about the troubleshooting and diagnostic
features.

7 Error Information
This chapter describes the meaning of error messages, and provides
information on probable causes and suggested actions how to recover from
error conditions.

Agilent InfinityLab LC Series DAD WR and MWD User Manual

3


In This Guide...

8 Test Functions and Calibration
This chapter describes the tests for the module.

9 Maintenance

This chapter describes the maintenance of the detector.

10 Parts for Maintenance
This chapter provides information on parts for maintenance and repair.

11 Identifying Cables
This chapter provides information on cables used with the Agilent 1200
Infinity Series modules.

12 Hardware Information
This chapter describes the detector in more detail on hardware and
electronics.

13 LAN Configuration
This chapter provides information on connecting the module to the Agilent
ChemStation PC.

14 Appendix
This chapter provides addition information on safety, legal and web.

4

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Contents

Contents

1 Introduction

9

Introduction to the Detector 10
G7115A Diode Array Detector WR 11
G7165A Multiple Wavelength Detector 13
Optical System 15
Leak and Waste Handling 18
Bio-inert Materials 23
2 Site Requirements and Specifications

25

Site Requirements 26
Physical Specifications 29
Performance Specifications 30
3 Using the Module

37

Magnets 38
Turn on/off 39
Status Indicators 40
Instrument Configuration 41
Set up the Detector with Agilent Open Lab ChemStation
The Detector User Interface 43
Detector Control Settings 45
Method Parameter Settings 46
4 Preparing the Detector

42

51

Leak and Waste Handling 52
Setting up an Analysis 54
Solvent Information 61

Agilent InfinityLab LC Series DAD WR and MWD User Manual

5


Contents

5 Optimizing the Detector

67

Optimizing the Detector Performance 68
Optimization Overview 69
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion
Optimizing Selectivity 81
Optimizing the Detector Regarding to the System 85
Warm up of the Detector 91
6 Troubleshooting and Diagnostics

93

Available Tests vs User Interfaces 94

Agilent Lab Advisor Software 95
Available Diagnostic Functions vs. Product Level
7 Error Information

71

96

99

What Are Error Messages 101
General Error Messages 102
Detector Error Messages 109
8 Test Functions and Calibration

117

Introduction 118
Conditions of Detector 122
Failing a Test 123
Self-Test 124
Intensity Test 126
Cell Test 129
Filter Test 132
Holmium Oxide Test 134
ASTM Drift and Noise Test 137
Slit Test 141
Wavelength Verification Test 144
Wavelength Calibration 146
D/A Converter (DAC) Test 149

Dark-Current Test 151
Spectral Scan 154
Other Lab Advisor Functions 155

6

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Contents

9 Maintenance

157

Introduction to Maintenance 158
Cautions and Warnings 159
Overview of Maintenance 161
Cleaning the Module 162
Remove and Install Doors 163
Replace a Lamp 164
Remove and Install a Flow Cell 168
Maintenance of Standard, Semi-Micro or Micro Flow Cell 172
Maintenance of High Pressure Flow Cell 176
Replacing Capillaries on a Standard Flow Cell 178
Replacing Capillaries on a Semi-Micro and Micro Flow Cell 183
Nano Flow Cell - Replacing or Cleaning 187
Cleaning or Exchanging the Holmium Oxide Filter 192
Correcting Leaks 195
Replacing Leak Handling System Parts 198

Replacing the Module’s Firmware 200
Information from Module’s Assemblies 202
10 Parts for Maintenance

203

Overview of Maintenance Parts 204
Standard Flow Cell 206
Standard Flow Cell Bio-inert 208
Semi-Micro Flow Cell 210
Micro Flow Cell 212
High Pressure Flow Cell 214
Prep Flow Cell - SST 216
Prep Flow Cell - Quartz 218
Nano Flow Cells 220
Accessory Kits 223
Holmium Oxide Filter 224
Leak Handling Parts 225

Agilent InfinityLab LC Series DAD WR and MWD User Manual

7


Contents

11 Identifying Cables

227

Cable Overview 228
Analog Cables 230
Remote Cables 232
BCD Cables 235
CAN/LAN Cables 237
Agilent 1200 module to PC
12 Hardware Information

238

239

Firmware Description 240
Electrical Connections 243
Interfaces 245
Setting the 6-bit Configuration Switch 252
Instrument Layout 255
Early Maintenance Feedback (EMF) 256
13 LAN Configuration

259

What You Have to Do First 260
TCP/IP parameter configuration 261
Configuration Switches 262
Initialization Mode Selection 263
Dynamic Host Configuration Protocol (DHCP)
Manual Configuration 268
14 Appendix

265

275

General Safety Information 276
Waste Electrical and Electronic Equipment Directive 282
Radio Interference 283
Sound Emission 284
UV-Radiation 285
Solvent Information 286
Declaration of Conformity for HOX2 Filter 287
Installation of Stainless Steel Cladded PEEK Capillaries 288
Agilent Technologies on Internet 295

8

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Agilent InfinityLab LC Series DAD WR and MWD User Manual

1
Introduction
Introduction to the Detector

10

G7115A Diode Array Detector WR
Product Description 11
Features 12

11

G7165A Multiple Wavelength Detector
Product Description 13
Features 14
Optical System

13

15

Leak and Waste Handling
Waste Concept 22
Bio-inert Materials

18

23

This chapter gives an introduction to the module.

Agilent Technologies

9


1

Introduction

Introduction to the Detector

Introduction to the Detector

The detector is designed for highest optical performance, GLP compliance and
easy maintenance. It includes the following features:
• 120 Hz data acquisition rate for (ultra-) fast LC applications,
• RFID tags for all flow cells and UV-lamps provides traceable information
about these assemblies,
• long-life deuterium with RFID tag and tungsten lamps for highest intensity
and lowest detection limit over a wavelength range of 190 – 950 nm,
• no loss in sensitivity for up to eight wavelengths simultaneous,
• programmable slit from 1 – 16 nm for complete optimization of sensitivity,
linearity and spectral resolution,
• optional flow-cell cartridges with RFID tag (standard 10 mm13 μL,
semi-micro 6 mm5 μL, micro 3 mm2 μL, 80 nL, 500 nL, 10 mm, high
pressure 10 mm1.7 μL and prep-cells) are available and can be used
depending on the application needs,
• easy front access to lamps and flow cell for fast replacement, and
• built-in holmium oxide filter for fast wavelength accuracy verification,
• built-in temperature control for improved baseline stability,
• additional diagnostic signals for temperature and lamp voltage monitoring,
For specifications, see “Specifications” on page 30.

10

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Introduction

G7115A Diode Array Detector WR

1

G7115A Diode Array Detector WR

Product Description
The 1260 Infinity II DAD WR detector is designed for highest optical
performance, GLP compliance, and easy maintenance. With its 120 Hz data
acquisition rate the detector is perfectly suited for fast LC applications. The
long –life deuterium lamps allow highest intensity and lowest detection limits
over a wavelength range of 190 – 950 nm. The use of RFID tags for all flow cells
and UV-lamps provides traceable information about these assemblies.
The built-in holmium oxide filter features the fast wavelength accuracy
verification, while the built-in temperature controls improves the baseline
stability. Additional diagnostic signals for temperature and lamp voltage
monitoring are available.
6WDWXVLQGLFDWRU
)ORZFHOO

3RZHUVZLWFK

/HDNGUDLQ

Figure 1

Overview of the detector

Agilent InfinityLab LC Series DAD WR and MWD User Manual

11


1

Introduction
G7115A Diode Array Detector WR

Features
• Higher sensitivity and selectivity - simultaneous detection of up to eight
compound-specific wavelengths.
• Low detection limits - low noise front-end electronics and the patented
flow cell design delivers very low detection limits thanks to the
minimization of short-term noise (< ± 7 μAU).
• Up to 100 % resolution gain in fast LC - using an 120 Hz data acquisition
rate.
• Maximum baseline stability - electronic temperature control (ETC)
reduces baseline drift under fluctuating ambient temperature and humidity
conditions.
• Wide linear range - for reliable, simultaneous quantification of primary
compounds, by-products, and impurities.
• Programmable slit (1 – 16 nm) for rapid optimization of sensitivity and
linearity.
• Excellent data traceability - radio frequency identification (RFID) tags on
cells and source lamps improve traceability of data.
• Automatic wavelength verification by built-in holmium oxide filter.
• Nine analytical and preparative flow cells provide you with maximum
application flexibility and choice.
• Extensive diagnostics, error detection and display with Instant Pilot
controller and Lab Advisor software.

12

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Introduction
G7165A Multiple Wavelength Detector

1

G7165A Multiple Wavelength Detector

Product Description
The 1260 Infinity II Multiple Wavelength Detector is designed for highest
optical performance, GLP compliance, and easy maintenance. With its 120 Hz
data acquisition rate, the detector is perfectly suited for fast LC applications.
The long-life deuterium lamps allows highest intensity and lowest detection
limits over a wavelength range of 190 – 950 nm. The use of RFID tags for all
flow cells and UV-lamps provides traceable information about these
assemblies.
The built-in holmium oxide filter features the fast wavelength accuracy
verification, while the built-in temperature controls improves the baseline
stability. Additional diagnostic signals for temperature and lamp voltage
monitoring are available.
6WDWXVLQGLFDWRU
)ORZFHOO

3RZHUVZLWFK

/HDNGUDLQ

Figure 2

Overview of the detector

Agilent InfinityLab LC Series DAD WR and MWD User Manual

13


1

Introduction
G7165A Multiple Wavelength Detector

Features
• Higher sensitivity and selectivity - simultaneous detection of up to eight
compound-specific wavelengths.
• Low detection limits - low noise front-end electronics and the patented
flow cell design delivers very low detection limits thanks to the
minimization of short-term noise (< ± 7 μAU).
• Up to 100 % resolution gain in fast LC - using a 120 Hz data acquisition
rate.
• Maximum baseline stability - electronic temperature control (ETC)
reduces baseline drift under fluctuating ambient temperature and humidity
conditions.
• Wide linear range - for reliable, simultaneous quantification of primary
compounds, by-products and impurities.
• Programmable slit (1 – 16 nm) for rapid optimization of sensitivity and

linearity.
• Excellent data traceability - radio frequency identification (RFID) tags on
cells and source lamps improve traceability of data.
• Automatic wavelength verification by built-in holmium oxide filter.
• Nine analytical and preparative flow cells provide you with maximum
application flexibility and choice.
• Extensive diagnostics, error detection and display with Instant Pilot
controller and Lab Advisor software.

14

Agilent InfinityLab LC Series DAD WR and MWD User Manual


1

Introduction
Optical System

Optical System

The optical system of the detector is shown in Figure below. Its illumination
source is a combination of a deuterium-arc-discharge lamp for the ultraviolet
(UV) wavelength range and a tungsten lamp for the visible (VIS) and
short-wave near-infrared (SWNIR) wavelength range. The image of the
filament of the tungsten lamp is focused on the discharge aperture of the
deuterium lamp by means of a special rear-access lamp design which allows
both light sources to be optically combined and share a common axis to the
source lens. The achromat (source lens) forms a single, focused beam of light
through the flow cell. Each cell room and lamp are separated by a quartz

window which can be cleaned or replaced. In the spectrograph, light is being
dispersed onto the diode array by a holographic grating. This allows
simultaneous access to all wavelength information.
&HOOVXSSRUWZLQGRZ
7XQJVWHQODPS
&RXSOLQJOHQV
'HXWHULXPODPS
$FKURPDWVRXUFHOHQV

+ROPLXPR[LGHILOWHU
)ORZFHOO
6SHFWUROHQV
6OLW
*UDWLQJ
'LRGHDUUD\

Figure 3

Optical System of the Detector

Agilent InfinityLab LC Series DAD WR and MWD User Manual

15


1

Introduction
Optical System
Lamps

Achromat
(Source Lens)

The light source for the UV-wavelength range is a deuterium lamp with a
shine-through aperture. As a result of plasma discharge in low-pressure
deuterium gas, the lamp emits light over the 190 nm to approximately 800 nm
wavelength range. The light source for the visible and SWNIR wavelength
range is a low noise tungsten lamp. This lamp emits light over the wavelength
range 470 – 950 nm.
The achromat receives the light from both lamps and focuses it so that the
beam passes through the flow cell.

Holmium Oxide
Filter

The holmium oxide filter is electromechanically actuated. During the holmium
filter test it moves into the light path.

Cell Support
Window

The cell support window assembly separates the holmium filter area from the
flow cell area.

Flow Cell
Compartment

The optical unit has a flow cell compartment for easy access to flow cells. A
variety of optional flow cells can be inserted using the same quick, simple

mounting system. The flow cell can be removed to check the optical and
electronic performance of the detector without having influences from the
flow cell.

Spectrograph

The spectrograph material is ceramic to reduce thermal effects to a minimum.
The spectrograph consists of the spectrograph lens, the variable entrance slit,
the grating and the photodiode array with front-end electronics. The
spectrograph lens refocuses the light beam after it has passed through the flow
cell. The sampling interval of the diode array is < 1 nm over the wavelength
range 190 – 950 nm. Depending on the wavelength this varies from 1.0 to 1.25
diodes per nanometer (for example a diode every 0.8 to 1 nm).
For a small wavelength range, the small non-linearity could be neglected. With
the wavelength range from 190 – 950 nm a new approach is required to
achieve wavelength accuracy over the full range. Each spectrograph is
calibrated individually. The calibration data is stored in the spectrograph on
an EEPROM. Based on these data, the built-in processors calculate absorbance
data with linear intervals (1.0, 2.0, …) between data points. This results in an
excellent wavelength accuracy and instrument-to-instrument reproducibility.

Variable Entrance
Slit System

16

The micro-slit system makes use of the mechanical properties of silicon
combined with the precise structuring capabilities of bulk micro-machining. It
combines the required optical functions — slit and shutter — in a simple and
compact component. The slit width is directly controlled by the

micro-processor of the instrument and can be set as method parameter.

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Introduction
Optical System

1

Grating

The combination of dispersion and spectral imaging is accomplished by using
a concave holographic grating. The grating separates the light beam into all its
component wavelengths and reflects the light onto the photodiode array.

Diode Array

The diode array is a series of 1024 individual photodiodes and control circuits
located on a ceramic carrier. With a wavelength range from 190 – 950 nm the
sampling interval is < 1 nm.

Agilent InfinityLab LC Series DAD WR and MWD User Manual

17


1

Introduction

Leak and Waste Handling

Leak and Waste Handling

The Agilent InfinityLab LC Series has been designed for safe leak and waste
handling. It is important that all security concepts are understood and
instructions are carefully followed.
The solvent cabinet is designed to store a maximum volume of 8 L solvent. The
maximum volume for an individual bottle stored in the solvent cabinet should
not exceed 2 L. For details, see the usage guideline for the Agilent 1200
Infinity Series Solvent Cabinets (a printed copy of the guideline has been
shipped with the solvent cabinet, electronic copies are available on the
Internet).
All leak plane outlets are situated in a consistent position so that all Infinity
and Infinity II modules can be stacked on top of each other. Waste tubes are
guided through a channel on the right hand side of the instrument, keeping the
front access clear from tubes.
The leak plane provides leak management by catching all internal liquid leaks,
guiding them to the leak sensor for leak detection, and passing them on to the
next module below, if the leak sensor fails. The leak sensor in the leak plane
stops the running system as soon as the leak detection level is reached.
Solvent and condensate is guided through the waste channel into the waste
container:
• from the detector's flow cell outlet
• from the Multisampler needle wash port
• from the Sample Cooler (condensate)
• from the Seal Wash Sensor
• from the pump's Purge Valve or Multipurpose Valve

18

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Introduction
Leak and Waste Handling

Figure 4

1

Infinity II Leak Waste Concept (flexible rack installation)

Agilent InfinityLab LC Series DAD WR and MWD User Manual

19


1

Introduction
Leak and Waste Handling

Figure 5

20

Infinity II Single Stack Leak Waste Concept (bench installation)

Agilent InfinityLab LC Series DAD WR and MWD User Manual

Introduction
Leak and Waste Handling

Figure 6

1

Infinity II Two Stack Leak Waste Concept (bench installation)

The waste tube connected to the leak pan outlet on each of the bottom
instruments guides the solvent to a suitable waste container.

Agilent InfinityLab LC Series DAD WR and MWD User Manual

21


1

Introduction
Leak and Waste Handling

Waste Concept
1 Agilent recommends using the 6 L waste can with 1 Stay Safe cap GL45
with 4 ports (5043-1221) for optimal and safe waste disposal. If you decide
to use your own waste solution, make sure that the tubes don't immerse in
the liquid.

22

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Introduction
Bio-inert Materials

1

Bio-inert Materials

For the Bio-inert LC system, Agilent Technologies uses highest quality
materials in the flow path (also referred to as wetted parts), which are widely
accepted by life science scientists, as they are known for optimum inertness to
biological samples and ensure best compatibility with common samples and
solvents over a wide pH range. Explicitly, the complete flow path is free of
stainless steel and free of other alloys containing metals such as iron, nickel,
cobalt, chromium, molybdenum or copper, which can interfere with biological
samples. The flow downstream of the sample introduction contains no metals
whatsoever.

Agilent InfinityLab LC Series DAD WR and MWD User Manual

23


1

Introduction

Bio-inert Materials

Table 1

Used Bio-inert materials

Module

Materials

Agilent 1260 Infinity II Bio-inert Pump
(G5654A)

Titanium, gold, platinum-iridium, ceramic,
ruby, PTFE, PEEK

Agilent 1260 Infinity II Bio-inert Multisampler
(G5668A)

Upstream of sample introduction:
• Titanium, gold, PTFE, PEEK, ceramic
Downstream of sample introduction:
• PEEK, ceramic

Agilent 1260 Infinity II Bio-inert Manual Injector
(G5628A)

PEEK, ceramic

Bio-inert Flow Cells:

Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar ( 12 MPa) for MWD/DAD,
includes Capillary Kit Flow Cells BIO (p/n G5615-68755) (G5615-60022)
(for Agilent 1260 Infinity II Diode Array Detectors DAD G7115A)

PEEK, ceramic, sapphire, PTFE

Bio-inert flow cell, 8 µL, 20 bar (pH 1–12) includes Capillary Kit Flow Cells BIO
(p/n G5615-68755) (G5615-60005)
(for Agilent 1260 Infinity Fluorescence Detector FLD G7121A/B)

PEEK, fused silica, PTFE

Quick-Connect Heat Exchanger Bio-inert (G7116-60041)
(for Agilent 1260 Infinity II Multicolumn Thermostat G7116A)

PEEK (steel-cladded)

Bio-inert Valve heads (G4235A, G5631A, G5632A, G5639A)

PEEK, ceramic (Al2O3 based)

Bio-inert Connection capillaries

Upstream of sample introduction:
• Titanium
Downstream of sample introduction:
• Agilent uses stainless-steel-cladded
PEEK capillaries, which keep the flow
path free of steel and provide
pressure stability to more than 600

bar.

NOTE

24

To ensure optimum bio-compatibility of your Agilent 1260 Infinity II Bio-inert LC system, do
not include non-inert standard modules or parts to the flow path. Do not use any parts that
are not labeled as Agilent “Bio-inert”. For solvent compatibility of these materials, see
“Material Information” on page 61.

Agilent InfinityLab LC Series DAD WR and MWD User Manual